ISSN: 0973-4945; CODEN ECJHAO

E-Journal of Chemistry
http://www.e-journals.net 2009, 6(1), 23-33

FTIR and Thermal Studies on Nylon-66 and

30% Glass Fibre Reinforced Nylon-66

JULIE CHARLES*, G. R. RAMKUMAAR,

S. AZHAGIRI and S. GUNASEKARAN

*
Dept. of Physics, S.S.N. College of Engineering,
Old Mahabalipuram Road, Kalavakkam 603 110, India.
Spectrophysics Research Laboratory,
PG and Research Dept. of Physics,
Pachaiyappas College, Chennai 600 030, India.
juliecharles2005@gmail.com

Received 24 May 2008; Accepted 20 July 2008

Abstract: The present study deals with the characterization of the polymeric
materials viz., nylon-66 and 30% glass fibre reinforced nylon-66 (GF Nylon-66)
by employing FTIR and thermal measurements. The complete vibrational band
assignment made available for nylon-66 and GF nylon-66 using FTIR spectra
confirm their chemical structure. FTIR spectroscopy provides detailed
information on polymer structure through the characteristic vibrational energies
of the various groups present in the molecule. The thermal behavior of nylon-66
and GF nylon-66 essential for proper processing and fabrication was studied from
TGA and DTA thermograms. The thermal stability of the polymers was studied
from TGA and the activation energy for the degradation of the polymeric
materials was calculated using Murray-White plot and Coats-Redfern plot. The
polymer with high activation energy is more thermally stable. GF nylon-66 is
found to be more thermally stable than nylon-66. The major thermal transitions
such as crystalline melting temperature (Tm) and degradation temperature (Td) of
the polymers were detected from DTA curves. The melting behaviour of the
polymer depends upon the specimen history and in particular upon the
temperature of crystallization. The melting behaviour also depends upon the rate
at which the specimen is heated. The various factors such as molar mass and
degree of chain branching govern the value of Tm in different polymers.

Keywords: Nylon-66, GF Nylon-66, FTIR spectra, Thermal stability, Activation energy, Thermal
transitions and Molecular symmetry.
24 JULIE CHARLES et al.

Introduction
Polymer characterization is an essential step in working with polymers. As a rule such efforts are
directed towards a specific purpose. The structure and organization of the macromolecules
ultimately determine the mechanical, physical and chemical properties of polymers1,2. Thus the
precise characterization of molecular order is a primary prerequisite to understanding the
macroscopic properties of polymeric materials3,4. The polymeric materials such as nylon-66 and
GF nylon-66 are studied here by utilizing important experimental techniques. The chemical
structure of the repeat unit of nylon-66 is presented in Figure 1. The polyamides were the first
engineering thermoplastics produced specifically by design as a plastic and are the largest family
in both production volume and number of applications. Nylon-66 is synthesized by condensation
polymerization of hexamethylenediamine and adipic acid. It is crystalline, and the crystals melt at
a high temperature. This makes it a good candidate for applications where properties such as high
strength, excellent chemical and abrasion resistance, and toughness are sought. In spite of its
superior properties, nylon-66 is very sensitive to moisture absorption5. Indeed, moisture content
must be controlled during melt processing of nylon-66.
There is however always a need to improve properties of nylon-66 to meet some
specific applications such as under-the-hood applications where humidity, high
temperature and repeated impact are encountered. One way to alter properties of
thermoplastics is to reinforce them with glass fibers6,7. There are several innate
characteristics of glass-fibers that make them ideal reinforcements. They have high tensile
strength to weight ratio and are perfect elastic materials (typical glass fibers have a
maximum elongation of 5% at break). They are incombustible (typical glass fibers retain
approximately 50% of their strength at 700F) and have a low thermal expansion
coefficient. They do not absorb moisture and are dimensionally stable.
Adding up to 40% by weight of glass fibers to nylon-66 increases strength and rigidity and
decreases the coefficient of thermal expansion. The most significant effect is the retention of
impact strength down to very low temperatures. In virtually all thermoplastics, impact
strengths at low temperatures improve with increasing glass fiber content. The heat distortion
temperature is improved most markedly in nylon, but less so in most other thermoplastics.
O O

C (CH2)4 C NH (CH2)6 NH
Diacid Diamine
n
Figure 1. Repeat unit of nylon-66
Experimental
The pure samples of nylon-66 and GF nylon-66 were obtained from Central Institute of Plastic
Engineering and Technology (CIPET), Chennai, India. The FTIR spectra have been recorded in
the range 4000-400 cm-1 using Bruker IFS 66V spectrophotometer at Indian Institute of
Technology (I.I.T), SAIF, Chennai, India. The standard sample preparation technique involves
making KBr discs, with finely ground polymer samples dispersed in the discs at concentrations of
less than 1%; they are prepared by compressing in a pellet-making press. The KBr discs with the
polymer sample were placed in the IR cell and the spectrum was recorded. IR is a useful and
highly specific tool8 to identify the chemical nature of the polymer and to determine its
composition. For quantitative analysis of microstructure, stereo regularity, branching or
crosslinking, in many cases, IR analysis is the simplest and most sensitive method.
 FTIR and Thermal Studies on Nylon-66 25

Thermoanalytical techniques are used for characterization of glass transition and

melting temperatures, thermal stability and other properties as a function of temperature of
polymers and fibres9. Thermogravimetric analysis was carried out in a high resolution
thermobalance (NETZSCH STA 409 C/CD instrument) at Indian Institute of Technology
(I.I.T), Chennai, India. TGA is a technique whereby the weight of a substance in an
environment is recorded when the sample is heated or cooled at a controlled rate and change
of weight is measured as a function of temperature or time. Approximately 5-6 mg of sample
was heated from room temperature to 1400oC at a heating rate of 20oC/min with a
continuous N2 flow. The sample weight and its rate of weight loss were continuously
measured as a function of temperature. The thermal stability of the selected polymeric
materials was studied from TGA curves.
DTA involves heating or cooling a test sample and an inert reference under identical
conditions, while recording any temperature difference between the sample and reference.
This differential temperature is then plotted against time, or against temperature. DTA
curves are recorded simultaneously with TGA curves. In the DTA trace, the baseline
remains unchanged so long as there is no thermal transition in the sample. First-order
transitions, namely crystallization (Tc) and melting (Tm), appear as peaks in the
exothermic and endothermic directions, respectively. After melting the material may
undergo decomposition reactions at higher temperatures (Td) which give broad peaks;
these may be generally exothermic but are sometimes more complex in shape10. The major
transition temperatures Tm and Td were detected from the DTA thermograms of nylon-66
and GF nylon-66.
Results and Discussion
Infrared spectroscopy is one of the most often used spectroscopic tools for the study of
polymers. Using FTIR spectroscopy, a lot of research work has been done in the recent past
for the study of polymers in various ways, e.g. identification of polymers and additives,
studies of coupling effects, conformational studies, stereochemical studies, studies relating
to crystalline forms, crystallinity of polymers and fibres, orientation in polymers and fibres
and end group analysis11,12. Polymeric blends of PVC and PET have been irradiated with 3
MeV proton beam and the radiation induced changes were investigated by N.L. Singh et al13
using FTIR spectroscopy. According to L.Z. Pillon et al14, FTIR has proven to be an
excellent technique to detect the presence of hydrogen bonding in the PET/nylon-66 blend.
Blends of PET and HDPE with and without a compatibilizing agent were studied by Carlos
Guerrero et al using infrared spectroscopy15.
IR spectroscopy has been usefully applied for identification of the basic structural units
present in the chemical configuration of nylon-66 and GF nylon-66. The FTIR spectra of the
polymeric materials are presented in Figures 2 and 3. The complete vibrational band
assignment is made available for the selected polymeric materials, thereby confirming their
molecular structure16. The vibrational frequencies of all the fundamental bands along with
their relative intensities and probable assignments are given in Tables 1 and 2. The primary
motivation for determining the molecular structure of a polymer using FTIR spectroscopy is
to relate the structures to the performance properties of the polymer in end use. If the
polymer chains are completely characterized and the structural basis of its properties are
known, the polymerization reaction can be optimized and controlled to produce the optimum
properties from the particular chemical system.
26 JULIE CHARLES et al.

%Transmission

Fig. 2 FTIR Spectrum of Nylon-66

Wave number, cm-1

Figure 2. FTIR spectrum of nylon-66
%Transmission

Figure 3. FTIR Spectrum of GF Nylon-66

Wave number, cm-1
Figure 3. FTIR spectrum of GF nylon-66
One of the important properties of polymeric materials is its thermal behavior. TGA is a
thermo analytical method used to study the thermal properties of elastomers. In this procedure,
the weight of a sample is continuously monitored as the sample temperature increases. When a
sample decomposes or degrades, normally the decomposition components volatilize off,
resulting in a change in weight. The continuous weight loss curves for the thermal degradation
of unfilled and glass fibre filled nylon are presented in Figures 4 and 5. The thermal stability
of the chosen rubber samples was studied from TGA. These thermograms suggest that the
samples are thermally stable up to 391oC. Thermal stability refers to the ability to maintain
required mechanical properties such as strength, toughness and elasticity at a given
temperature. It is also used to determine the kinetic parameters of degradation of rubber
materials. The thermal stability of the selected rubber materials at different temperatures are
presented in Table 3.
 FTIR and Thermal Studies on Nylon-66 27

Table 1. FTIR spectra and assignment of nylon-66

Frequency, cm-1
Assignment
FTIR Intensity
3182 m N-H stretching
3080 ms C-H asymmetric stretching
3020 m C-H symmetric stretching
2958 ms CH2 asymmetric stretching
2841 ms CH2 symmetric stretching
1745 vs C=O stretching
1660 vs Amide I band
1541 vs Amide II band/CH2 asymmetric deformation
1447 vs N-H deformation/CH2 scissoring
1354 vs Amide III band/CH2 wagging
1149 vs CCH symmetric bending/CH2 twisting
1128 vs CCH symmetric bending
959 ms C-C stretching
755 w N-H wagging/CH2 rocking
606 s C-C bending
549 vw O=C-N bending
vs-very strong s-strong ms-medium strong m-medium w-weak
Table 2. FTIR spectra and assignment of glass filled nylon-66
Frequency, cm-1
Assignment
FTIR Intensity
3260 vs N-H stretching
3070 vs C-H asymmetric stretching
2920 vs CH2 asymmetric stretching
2856 vs CH2 symmetric stretching
1716 vs C=O stretching
1630 vs Amide I band
1522 vs Amide II band/ CH2 asymmetric deformation
1456 vs N-H deformation/CH2 scissoring
1355 vs Amide III band/CH2 wagging
1142 w CCH symmetric bending/CH2 twisting
1014 m C-C stretching
820 vvw N-H wagging
723 vw CH2 rocking
568 w C-C deformation
547 w O=C-N bending
vs-very strong s-strong ms-medium strong m-medium w-weak
Table 3. Thermal stability of polymeric materials
Temperature, oC corresponding to weight loss
Sample
10% 20% 30% 40% 50% 60% 70% 80% 90%
Nylon-66 392 419 431 441 448 454 495 - -
GF Nylon-66 403 422 434 443 453 460 - - -
28 JULIE CHARLES et al.

TG%

Temperature, oC

Figure 4. TGA thermogram of nylon-66

TG%

Temperature, oC
Figure 5. TGA thermogram of GF nylon-66
The degradation process is single stage for nylon-6617 and 30% glass fibre reinforced nylon-
66. Both the polymers have undergone 63% decomposition in this stage. Between 366oC and
495oC, 63% of nylon-66 was degraded. 63% of glass filled nylon-66 was degraded between
340oC and 502oC. The degradation temperatures corresponding to 30% and 60% weight losses
are 431oC and 454oC for nylon-66. The TGA curve of glass filled nylon-66 shows a weight loss
of 30% at 434oC and 60% at 460oC. Unfilled nylon degrades at slightly lower temperatures than
glass filled nylon. Further nylon-66 undergoes 70% degradation at 495oC. This means that glass
filled nylon is thermally more stable than unfilled nylon. On the whole 75% of nylon-66 gets
degraded and 67% of glass filled nylon-66 gets degraded at 1400oC which further confirms that
glass filled nylon-66 is thermally more stable than unfilled nylon-66.
Activation energies of degradation of polymeric materials
Activation energy is the minimum amount of energy that is required to activate atoms or
molecules to a condition in which they can undergo chemical transformation or physical
transport. Activation energy calculations for the degradation of nylon-66 and GF nylon-66
were made from TGA curves using Murray-White plot18 and Coats-Redfern plot19. A linear
 FTIR and Thermal Studies on Nylon-66 29

correlation was obtained by plotting the logarithm of heating rate against the reciprocal of
the absolute temperature. In Murray-White method, a linear correlation was obtained by
plotting T-1X10-3 (K-1) against [ln(ln(1-C)-2lnT]. In Coats-Redfern method, a linear
correlation was obtained by plotting T-1X10-3 (K-1) against log[ln(1-C)]/T2. The method of
calculating activation energy20,21 for the degradation of nylon-66 and GF nylon-66 are given
in Tables 4 and 5. The Arrhenius plot for degradation of polymers using Murray-White plot
and Coats-Redfern plot is presented in Figure 6. Activation energy calculated from TGA
curve using the two methods is presented in Table 6.
Murray and White Method
T-1x10-3 (K-1) Vs ln [ln (1-C)] -2ln T
- 11. 4 5 -11.5

- 11. 5 Nylon -11.55 GF Nylon

- 11. 5 5 -11.6

-11.65
- 11. 6

-11.7
- 11. 6 5
y axis

y axis

-11.75
- 11. 7

-11.8
- 11. 7 5

-11.85
- 11. 8

-11.9
- 11. 8 5

-11.95
- 11. 9 1.35 1.4 1.45 1.5
1. 3 5 1. 4 1. 4 5 1. 5 1. 5 5
x-axis
x - ax is

Coats and Redfern Method

T-1x10-3 (K-1) Vs log [ln (1-C)] / T2
1.6 1.5

1.5 1.45

1.4
1.4
Nylon 1.35 GF Nylon
1.3
1.3

1.2
y axis

1.25
y axis

1.1 1.2

1 1.15

1.1
0.9
1.05
0.8
1
1.35 1.4 1.45 1.5 1.55
1.35 1.4 1.45 1.5
x- axis x-axis

Figure 6. Arrhenius plot of degradation of polymer materials

30 JULIE CHARLES et al.

Table 4. Calculation of activation energy for the degradation of nylon-66

T T-1 x 10-3 ln[ln(1-C)] log[ln(1-C)]
Degradation% 1-C 2lnT T2
K K-1 -2lnT /T2 X 106
10 665 1.5037 90 12.9995 442225 -11.4955 1.476
20 692 1.4450 80 13.0791 478864 -11.6016 1.339
30 704 1.4204 70 13.1135 495616 -11.667 1.267
40 714 1.4005 60 13.1417 509796 -11.7322 1.2
50 721 1.3869 50 13.1612 519841 -11.7972 1.139
60 727 1.3755 40 13.1778 528529 -11.8725 1.072
Table 5. Calculation of activation energy for the degradation of 30% GF nylon-66
% T T-1x10-3 ln[ln(1-C)]- log[ln(1-C)]
1-C 2lnT T2
Degradation K K-1 2lnT /T2 X 106
10 676 1.4792 90 13.0323 456976 -11.5283 1.429
20 695 1.4388 80 13.0878 483025 -11.6103 1.328
30 707 1.4144 70 13.1220 499849 -11.6755 1.256
40 716 1.3966 60 13.1473 512656 -11.7378 1.193
50 726 1.3774 50 13.1751 527076 -11.8111 1.123
60 733 1.3642 40 13.1942 537289 -11.8889 1.054
Table 6. Activation energy for the degradation of polymer materials
Activation energy Ea in kJ/mol
Sample
Murray-White Method Coats-Redfern Method
Nylon-66 0.1427 0.2169
GF Nylon-66 0.4189 0.5021
It is evident from Table 6, Glass filled Nylon-66 has high decomposition activation
energy than unfilled nylon-6617. TGA curves show that glass filled nylon degrades at
slightly higher temperatures than unfilled nylon. Moreover, 25% of unfilled nylon remains
undecomposed whereas 33% of glass filled nylon remains as a residue material. Thus, the
polymeric materials with high activation energy are more thermally stable which is
supported by 22,23.
The DTA curves for the polymers are shown in Figures 7 and 8. The major transition
temperatures such as crystalline melting temperature (Tm) and degradation temperature (Td)
were identified from DTA curves of polymers. There are several characteristics of the
melting behaviour of polymers which distinguishes them from other materials. It is not
possible to define a single melting temperature for a polymer sample as the melting
generally takes place over a range of temperature. The melting behaviour depends upon the
specimen history and in particular upon the temperature of crystallization and the rate at
which the specimen is heated24. There is found to be a strong dependence of the observed
melting temperature of a polymer crystal, Tm, upon the crystal thickness l. A process which
affects the melting behaviour of crystalline polymers and is of interest in its own right is
annealing. It is found that when crystalline polymers are heated to temperatures just below
the melting temperature, there is an increase in lamellar crystal thickness. The driving force
is the reduction in free energy gained by lowering the surface area of a lamellar crystal when
it becomes thicker and less wide. The lamellar thickening only happens at relatively high
temperatures when there is sufficient thermal energy available to allow the necessary
molecular motion to take place. A certain amount of annealing usually takes place when a
 FTIR and Thermal Studies on Nylon-66 31

crystalline polymer sample is heated and melted. The increase in lamellar thickness,
l, causes an increase in Tm. This means that the measured melting temperature will depend
upon the heating rate because annealing effects will be lower for more rapid rates of heating.
DTA/mW/mG

Temperature, oC
Figure 7. DTA thermogram of nylon-66
DTA/mW/mG

Temperature, oC
Figure 8. DTA thermogram of GF nylon-66
The important thermal transitions such as Tm and Td detected from DTA curves are
presented in Table 7. The use of polymers in many practical applications is often limited by
their relatively low melting temperatures. Because of this there has been considerable interest
in determining the factors which control the value of Tm and in synthesizing polymers which
have high melting temperatures25. For a particular type of polymer the value of Tm depends
upon the molar mass and degree of chain branching. Chain ends and branches can be thought
of as impurities which depress the melting points of polymer crystals. In 1882, Thomas
Carnelley observed that high molecular symmetry is associated with high melting point26.
Symmetrical molecules in crystalline form have higher melting temperatures and exhibit lower
solubility compared with molecules of similar structure but with lower symmetry. Symmetry
32 JULIE CHARLES et al.

in a molecule imparts a positive amount of residual entropy in the solid phase. This means that
the entropy of a substance of symmetric molecules is greater than the entropy of substance of a
similar, but non-symmetric molecule. Hence, it is concluded from Table 7 that GF Nylon with
high crystalline melting point has high molecular symmetry, low solubility and high entropy.
Table 7. Thermal transition of polymers
Peak Temperature, oC
Sample
Tm Td
Nylon-66 171.3 366 495
GF Nylon-66 215.6 395 502
Conclusion
The characterization studies on nylon and glass fibre reinforced nylon have been carried out
using important experimental techniques. Their molecular structure was confirmed using FTIR
spectroscopic technique. Once the molecular structure of a polymer is understood using FTIR
spectroscopy, it becomes easy for a polymer scientist to relate the polymer structure to its
performance properties in end use. The thermal stability of the polymeric materials was studied
using TGA thermograms. The thermal study shows that glass fibre reinforced nylon is more
thermally stable than unfilled nylon. The activation energy was calculated in KJ/ mol for the
degradation of polymers using Murray-White method and Coats-Redfern method. GF Nylon
is found to have high activation energy calculated using both the methods. Since high
decomposition activation energy is associated with high thermal stability, GF Nylon is
considered to be more thermally stable than unfilled nylon. Finally, the major transition
temperatures Tm and Td were identified from DTA curves. The higher Tm value indicates the
crystalline nature of the polymer. This means that at room temperature, GF Nylon has a high
degree of crystallinity than unfilled nylon. Thus it is concluded that the elastomers with high
melting point have high molecular symmetry, low solubility and high entropy.
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